甲基肼合成新工艺

以亚磷酸二甲酯为甲基化试剂 ,一步合成了单取代的一甲基肼。在优化反应条件下 ,水合肼的转化率高于 63.68% ,甲基肼的收率高达 5 1 .5 8%。优化反应条件如下 :水合肼和亚磷酸二甲酯的摩尔比为 1 .0∶ ( 1 .2～ 1 .3) ,反应时间 3～ 4h,反应温度为 1 30～ 1 40℃ ,实验结果表明此工艺反应条件温和、方法简单易行、收率较高 ,为工业化生产提供了依据。并通过实验证明了加料方式对合成反应的影响较大。

A New Synthetic Technology of Monomethylhydrazine

The synthesis of monomethylhydrazine was investigated with dimethyl phosphite as methylating agent. Under optimum conditions the conversion yield of hydrazine was up to 63.68%, the yield of monomethylhydrazine reached 51.58%. The conditions were as follows: molar ratio of hydrazine to dimethyl phosphite=1.0∶(1.2～1.3) reaction time:3～4 h, reaction temperature: 130～140℃. The experiment indicated that the reaction conditions were suitable, the method was simple and feasible, and the yield of monomethylhydrazine was quite high. Thus, it provides the basis to industrialization. It was found that feeding manner obviously influencing the yield.